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Perfluoropolyether and preparation method thereof

A perfluoropolyether, polymerization technology, applied in chemical instruments and methods, chemical/physical/physical chemical processes, chemical/physical processes, etc., can solve the problems of reduced reaction efficiency, strong glass corrosion, and blurred glass corrosion. , to achieve high reaction efficiency, stable temperature control, and good product quality.

Active Publication Date: 2020-09-04
浙江创氟高科新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (2) Perfluoropolyether intermediates generally contain more acyl fluoride groups. At the same time, carbonyl fluoride and other substances will be generated during the process. These substances are easy to form HF when they meet water, and HF is extremely corrosive to glass. UV Photodecomposition of peroxides will cause corrosion and blurring of the external glass of the light source, reducing reaction efficiency

Method used

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  • Perfluoropolyether and preparation method thereof
  • Perfluoropolyether and preparation method thereof
  • Perfluoropolyether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put hexafluoropropylene, oxygen and the solvent perfluorocyclic ether into the degassing tower after photoinitiated reaction, degassing at 30°C for 1 hour, and the by-products (low molecular weight perfluoroalkyl fluoride, etc.) The oxygen after the reaction is removed. The degassed reaction solution (perfluoropolyether intermediate product content is 23.33wt%) enters the corning "heart-shaped" silicon carbide microchannel with a metering pump at 30g / min (perfluoropolyether intermediate product feed rate 7g / min) Into the reactor, tetrafluoroethylene monomer (A=F) was simultaneously fed in at a gas rate of 2.0 g / min. The microchannel reactor includes 1 mixing module, 5 reaction modules, and 6 heat transfer modules. The channel equivalent diameter of the mixing module is 100 μm, the channel equivalent diameter of the reaction module is 100 μm, and the channel equivalent diameter of the heat transfer module is 100 μm. Control reaction temperature 85 ℃, reaction pressure 2...

Embodiment 2

[0039]Put hexafluoropropylene, oxygen and the solvent perfluorocyclic ether into the degassing tower after photoinitiated reaction, degassing at 30°C for 1 hour, and the by-products (low molecular weight perfluoroalkyl fluoride, etc.) The oxygen after the reaction is removed. The degassed reaction solution (perfluoropolyether intermediate product content is 23.33wt%) enters the corning "heart-shaped" silicon carbide microchannel with a metering pump at 30g / min (perfluoropolyether intermediate product feed rate 7g / min) Into the reactor, tetrafluoroethylene monomer (A=F) was fed at the same time at a gas rate of 2.33 g / min. The microchannel reactor includes 1 mixing module, 6 reaction modules, and 3 heat transfer modules. The channel equivalent diameter of the mixing module is 500 μm, the channel equivalent diameter of the reaction module is 500 μm, and the channel equivalent diameter of the heat transfer module is 500 μm. The reaction temperature was controlled at 80° C. and t...

Embodiment 3～9

[0041] The reaction liquid obtained after photoinitiated reaction of hexafluoropropylene, oxygen and solvent enters the degassing tower, degasses at 30°C for 1 hour, and degasses by-products (low molecular weight perfluoroalkyl fluoride, etc.) and unreacted oxygen remove. The degassed reaction solution is fed into the corning "heart-shaped" silicon carbide microchannel reactor at a rate of 30 g / min by a metering pump, and different fluorine-containing monomers (A is a different group) are fed in at a certain rate at the same time. The microchannel reactor includes 1 mixing module, 7 reaction modules, and 5 heat transfer modules. The channel equivalent diameter of the mixing module is 1000 μm, the channel equivalent diameter of the reaction module is 1000 μm, and the channel equivalent diameter of the heat transfer module is 1000 μm. Certain reaction temperature, control certain reaction pressure. The reaction conditions and results are shown in Table 1.

[0042] Summary of r...

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Abstract

The invention discloses a perfluoropolyether and a preparation method thereof. The preparation method comprises the following steps: degassing a reaction solution containing a perfluoropolyether intermediate product obtained by oxidative polymerization of fluorine-containing olefin, carrying out polymerization reaction on the degassed reaction solution and a fluorine-containing monomer, and carrying out desolvation on the obtained reaction product to separate a solvent, thereby obtaining a perfluoropolyether product. The method has the advantages of high efficiency, continuity and safety.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a perfluoropolyether and a preparation method thereof. Background technique [0002] Perfluoropolyether (PFPE) is a polymer with only three elements of C, F, and O in the molecule, and it is liquid at room temperature. There are stronger C-F bonds in PFPE molecules instead of C-H bonds in hydrocarbons, and due to the existence of C-O and C-C strong covalent bonds, as well as the neutral characteristics of PFPE molecules, PFPE has higher chemical stability and oxidation stability. and good chemical inertness and insulating properties. This type of perfluoropolyether has a wide range of potential uses. For example, when the terminal group is fluorinated to form a stable -CF3 group, it can be used as a perfluoropolyether oil; when the terminal group is hydrolyzed to form -COOH, it can be used as a Emulsifier, widely used in oil field, paint, fluoropolymer emulsifier an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F114/26C08F116/14C08F114/24C08F2/01B01J19/00
CPCC08F114/26C08F116/14C08F114/24C08F2/01B01J19/0093
Inventor 吴庆耿为利郑磊马利勇
Owner 浙江创氟高科新材料有限公司
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